• 제목/요약/키워드: Reaction ball milling

검색결과 101건 처리시간 0.025초

리튬이차전지용 탄소 코팅된 Li2MnSiO4 양극활물질의 상형성 거동 및 충방전 특성 (Phase Formation Behavior and Charge-discharge Properties of Carbon-coated Li2MnSiO4 Cathode Materials for Lithium Rechargeable Batteries)

  • 선호정;채수만;심중표
    • 전기화학회지
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    • 제18권4호
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    • pp.143-149
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    • 2015
  • Planetary ball mill과 고상반응법을 사용하여 실리케이트계 탄소 코팅된 $Li_2MnSiO_4$ 양극활물질 분말을 합성하였으며 충방전 특성을 조사하였다. 전기화학적 활성을 지니는 ${\beta}-Li_2MnSiO_4$ 상을 형성하기 위하여 하소 온도와 분위기를 조절하였으며 ${\beta}-Li_2MnSiO_4$ 단일상에 가까운 탄소 코팅된 $Li_2MnSiO_4$ 활물질 분말을 제조할 수 있었다. 합성된 분말은 100 nm 정도 크기의 1차 입자가 뭉쳐있는 2차 입자 형태를 보였다. $Li_2MnSiO_4$ 활물질에서 Li의 삽입/탈리가 가능하려면 탄소의 첨가가 필요하였으며, 4.8 wt%의 탄소가 코팅된 $Li_2MnSiO_4$ 활물질에서 초기용량 192 mAh/g를 얻을 수 있었다.

기계적 합금화과정에서의 in situ 열분석에 의한 Ti-25.0~37.5at%Si 분말의 합성거동 (Synthesis Behavior of Ti-25.0~37.5at%Si Powders by In situ Thermal Analysis during Mechanical Alloying)

  • 변창섭;현창용;김동관
    • 한국재료학회지
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    • 제14권5호
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    • pp.305-309
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    • 2004
  • Mechanical alloying (MA) of Ti-25.0~37.5at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-25.0~26.1at%Si powders showed that there were no peaks during MA, indicating $Ti_{5}$ $Si_3$ was synthesised by a slow reaction of solid state diffusion. Those of Ti-27.1~37.5at%Si powders, however, showed that there were exothermic peaks during MA, indicating $_Ti{5}$ $Si_3$ and$ Ti_3$Si phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). For Ti-27.1~37.5at%Si powders, the critical milling times for SHS decreased from 38.1 to 18.5 min and the temperature rise, ΔT (= peak temperature - onset temperature) increased form $19.5^{\circ}C$ to $26.7^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 27.1at% and the critical value of the negative heat of formation of Ti-27.1at%Si to be -1.32 kJ/g.

기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화 (Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders)

  • 이충효;전성용;김지순
    • 한국결정성장학회지
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    • 제14권4호
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    • pp.129-134
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    • 2004
  • 본 연구에서는 기계적 합금화(MA)에 의한 고상-기상반응에 있어서 질소원자가 V-Fe계 합금의 비정질화에 미치는 영향을 조사하였다. 유성형 볼밀을 사용하여 $V_{70}Fe_{30}$혼합분말을 질소가스 분위기 중 MA 처리하였다. 그 결과 160시간 MA 처리에 의하여 비정질상이 생성됨을 알 수 있었다. 160시간 동안 MA 처리한 ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ 분말시료의 열분석 결과 약 $600^{\circ}C$에 비정질상의 결정화에 의한 발열 peak가 관찰되었다. 또한 bcc 결정에서 비정질상으로의 구조변화 과정을 X선 및 중성자 회절법을 통하여 조사하였으며, 특히 중성자회절에서는 V원자의 중성자에 대한 간섭성 핵산란진폭이 매우 작은 특징을 이용하였다. 그 결과, 이 합금계에서의 비정질화는 모든 결정구조에서 전형적으로 존재하는 8면체 unit가 우선적으로 붕괴되어 4면체 unit로 변환되어 가는 과정임을 알 수 있었다. 또한 중성자 회절에 의한 구조해석 결과 질소원자는 V원자로 이루어진 다면체의 중심에 위치하고 있음을 알 수 있었다.

(Fe, TiH2, C) 혼합 분말로부터 제조된 Fe-30 wt% TiC 복합재료 분말의 소결 (Sintering of Fe-30 wt% TiC Composite Powders Fabricated from (Fe, TiH2, C) Powder Mixture)

  • 이병훈;김지순
    • 한국분말재료학회지
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    • 제22권5호
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    • pp.356-361
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    • 2015
  • Fe-30 wt% TiC composite powders are fabricated by in situ reaction synthesis after planetary ball milling of (Fe, $TiH_2$, Carbon) powder mixture. Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe-30 wt% TiC composite powder compacts. Pressureless sintering is performed at 1100, 1200 and $1300^{\circ}C$ for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of $1050^{\circ}C$, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of $50^{\circ}C/min$, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts are not densified even after sintering at $1300^{\circ}C$ for 3 h, which shows a relative denstiy of 66.9%. Spark-plasma sintering at $1050^{\circ}C$ for 10 min exhibits nearly full densification of 99.6% relative density under the sintering pressure of 50 MPa.

광흡수층 적용을 위한 PLD용 $Cu_2ZnSnSe_4$ 타겟 제조와 증착 박막의 특성 (Characteristics of $Cu_2ZnSnSe_4$ Thin Film Solar Absorber Prepared by PLD using Solid Target)

  • 정운화;라흐멧 아드히 위보우;김규호
    • 한국신재생에너지학회:학술대회논문집
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    • 한국신재생에너지학회 2009년도 춘계학술대회 논문집
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    • pp.130-133
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    • 2009
  • $Cu_2ZnSnSe_4$(CZTSe) is one of the promising materials for the solar cell due to its abundant availability in the nature. In this study, we report the fabrication of CZTSe thin film by Pulsed Laser Deposition(PLD) method using quaternary compound target on sodalime glass substrate. The quaternary CZTSe compound target was synthesized by solid state reaction method using elemental powders of Cu, Zn, Sn and Se. Powders were milled in high purity ethanol using zirconia ball with mixed size of 1 and 3 mm at the same proportions for 72 hours milling time. The structural, chemical and mechanical properties of the synthesized CZTSe powders were investigated prior to the deposition process. The CZTSe compound powder, and $500^{\circ}C$ of sintering temperature shows the best properties for PLD target. Results show that the as-deposited CZTSe thin films with the precursors by PLD have a composition near-stoichiometric.

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타이타늄 하이드라이드 분말의 침탄에 의한 타이타늄 카바이드 분말 제조 (Fabrication of TiC powder by carburization of TiH2 powder)

  • 이훈석;서향임;이영선;이동준;왕제필;이동원
    • 한국분말재료학회지
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    • 제24권1호
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    • pp.29-33
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    • 2017
  • Titanium carbide (TiC) powders are successfully synthesized by carburization of titanium hydride ($TiH_2$) powders. The $TiH_2$ powders with size lower than $45{\mu}m$ (-325 Mesh) are optimally produced by the hydrogenation process, and are mixed with graphite powder by ball milling. The mixtures are then heat-treated in an Ar atmosphere at $800-1200^{\circ}C$ for carburization to occur. It has been experimentally and thermodynamically determined that the de-hydrogenation, "$TiH_2=Ti+H_2$", and carburization, "Ti + C = TiC", occur simultaneously over the reaction temperature range. The unreacted graphite content (free carbon) in each product is precisely measured by acid dissolution and by the filtering method, and it is possible to conclude that the maximal carbon stoichiometry of $TiC_{0.94}$ is accomplished at $1200^{\circ}C$.

Enzymatic Hydrolysis of Pretreated Chitin by Aspergillus carneus Chitinase

  • Mohamed, Abdel-Naby;Kwon, Dae-Young
    • Journal of Microbiology and Biotechnology
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    • 제2권3호
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    • pp.197-203
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    • 1992
  • Studies of the pretreatment of chitin and its subsequent hydrolysis by Aspergillus carneus chitinase are reported. Ball milling was found to be the most effective way among the pretreatment methods tested. Data are presented describing the effect of enzyme and substrate concentrations on the rate and extent of the hydrolysis process. It was found that the successive addition of enzyme improved the saccharification yield. Significant product inhibition of the chitinase was observed when N-acetylglucosamine concentration was 3.6% or higher. Adsorption of enzymes to the substrate occurred during a 24 hr hydrolysis period. An initial rapid and extensive adsorption occurred, followed by gradual desorption which increased during the time of reaction. Intermediate removal of the hydrolyzate and continuation of the hydrolysis by adsorbed enzyme on the residual chitin was also investigated. A total of 75.4 g/l reducing sugars, corresponding to 69.2% saccharificaton yield (as N-acetylglucosamine) was obtained. In addition an increase in the amount of recoverable enzymes was observed under these conditions. Evidence presented here suggests that the technique, whereby the free enzymes in the recovered hydrolyzate are re-adsorbed onto the new substrate, may provide a means of recirculating the dissolved enzymes.

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입자분쇄 시간변화에 따른 압전세라믹스 제작공정과 특성 분석 (Processing and Characterization of Piezoelecteric Geramics Depending on Ball Milling Time)

  • 박종호;배숙희;김철수;송석천;허창회;이상렬
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 2000년도 추계학술대회 논문집 학회본부 C
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    • pp.413-415
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    • 2000
  • Piezoelectric ceramics of PZT have been developed to apply for transformers in notebook. Use of piezoelectric ceramics in applications like piezoelectric transformers was made possible by the development of new materials with high electromechanical coupling coefficients and high mechanical quality factor. "Hard" ferroelectiric ceramics of complex composition based on lead zirconate titanate with Mn additive have been prepared. The perovskitic phase reaction of the oxides. The crucial role played by the intermediate mixing and grinding procedures in the assessment of the final properties of the material was investigated. Densification up to approximately the theoretical density value was achieved. The polarization was obtained by subjecting the samples at $30kVcm^{-1}$ poling electric field, in a silicon oil bath heated at $110^{\circ}C$. Their microstructural and morphological properties were checked by X-ray diffraction analysis and scanning electron microscopy. The optimized samples presented very high qualify and electromechanical coupling factors, together with small dielectric loss.

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Hybrid Sol을 이용한 박막 유전체 제작 (Fabrication of Thin Film Dielectric by Hybrid Sol)

  • 김용석;유원희;장병규;오용수
    • 한국재료학회지
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    • 제17권4호
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    • pp.185-191
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    • 2007
  • The purpose of this study is to evaluate the thin fihn dielectric made of hybrid sol, which consist of barium titanate powder, polymeric sol and other polymers. This sol will be used dielectric applied to small, thin electric passive components such as MLCC(Multi Layer Ceramic Condenser), resister, inductor. This sol is composed of mixed fine barium titanate powder and polymeric sol including Ba, Ti-precursor, solvent, chelating agent, chemical reaction catalyst, the additive sols to improve fired densification and temperature reliability. First at all, we mixed hybrid sol to be dispersed and be stabilized by ball milling for 24hrs. By spin coating method, we makes thin film dielectric on the convectional green sheet for MLCC. After heat treatments, we analyzes the structure morphology, physical, electrical properties and X5R Temperature properties.

마그네타이트와 금속(Ti, Al)의 기계적 합금화에 의한 복합분말의 합성 (Fabrication of Composite Powders by Mechanical Alloying of Magnetite-M (M = Ti, Al) Systems)

  • 홍대석;이성희;이충효;김지순;권영순
    • 한국분말재료학회지
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    • 제11권3호
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    • pp.247-252
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    • 2004
  • Recently, it has been found that mechanical alloying (MA) facilitates the nanocomposites formation of metal-metal oxide systems through solid-state reduction during ball milling. In this work, we studied the MA effect of Fe$_{3}$O$_{4}$-M (M = Al, Ti) systems, where pure metals are used as reducing agents. It is found that composite powders in which $Al_{2}$O$_{3}$ and TiO$_{2}$ are dispersed in $\alpha$-Fe matrix with nano-sized grains are obtained by mechanical alloying of Fe$_{3}$O$_{4}$ with Al and Ti for 25 and 75 hours, respectively. It is suggested that the large negative heat associated with the chemical reduction of magnetite by aluminum is responsible for the shorter MA time for composite powder formation in Fe$_{3}$O$_{4}$-Al system. X-ray diffraction results show that the reduction of magnetite by Al and Ti if a relatively simple reaction, involving one intermediate phase of FeAl$_{2}$O$_{4}$ or Fe$_{3}$Ti$_{3}$O$_{10}$. The average grain size of $\alpha$-Fe in Fe-TiO$_{2}$ composite powders is in the range of 30 nm. From magnetic measurement, we can also obtain indirect information about the details of the solid-state reduction process during MA.